Standardisierung quantitativer Analysenverfahren

Prevalidation in pharmaceutical analysis

“…For full prevalidation process N = 24, and for exploratory prevalidation this number is 8. Number of observations covered by N = 24 measurements was based on six analytical groups (J = 6), each of the volume of four replicates of identical properties of the sample (I = IV) [13,43]. It was shown in practice that four parallel measurements were good choice in analysis [13] and this is confirmed recently by statement that each calibration level must be treated at least as triplicates in evaluation of the limit of quantitation [1].…”

“…According to almost the same principle, analytical evaluation function was established starting from parabolic function:x = U + VS + WS 2 (R14, Table 5) using algorithms presented in detail in papers [13,43].…”

“…As prevalidation concept presumes that the second degree polynomial is sufficient condition for the description of analyte-signal relationship in great number of analytical procedures, Gottschalk approach [13] was used. The calculations for both calibration and analytical evaluation functions were based on sums and determinants as it was given in R13 (Table 5).…”

“…Number of observations covered by N = 24 measurements was based on six analytical groups (J = 6), each of the volume of four replicates of identical properties of the sample (I = IV) [13,43]. It was shown in practice that four parallel measurements were good choice in analysis [13] and this is confirmed recently by statement that each calibration level must be treated at least as triplicates in evaluation of the limit of quantitation [1]. In instrumental analyses, in which the fluctuation of working parameters is occurred, it is recommended to perform two successive measurements of the same analyte solution (an average value of those two measurements is used for further calculation).…”

“…published by a number of bodies [2][3][4][5][6][7]. The key literature to this subject is valuable paper from Ermer [8], the former discussions on complete analytical procedure [9][10][11], and papers on standardization of quantitative analytical procedure [12][13][14][15][16].…”